Dipotassium bismuth phosphate tungstate has been synthesized using the flux technique. It crystallizes in the space group Ibca and is isotypic with Na2Y(PO4)(MoO4). It exhibits a layered structure, which is built up from [Bi(PO4)(WO4)]∞2− layers. Each layer is composed of [BiO8]∞ zigzag chains, which are connected via PO4 and WO4 tetrahedra. The parallel anionic [Bi(PO4)(WO4)]∞2− layers are stacked along [100] and are held together by K+ counter-cations which occupy sites in the interlayer space. Bi, W and P atoms are all located on twofold axes.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (P-O) = 0.006 Å
- R factor = 0.035
- wR factor = 0.094
- Data-to-parameter ratio = 20.4
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.06
Alert level G
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
1 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
1 ALERT type 2 Indicator that the structure model may be wrong or deficient
0 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: CrysAlis CCD (Oxford Diffraction, 2005); cell refinement: CrysAlis CCD; data reduction: CrysAlis RED (Oxford Diffraction, 2005); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: WinGX (Farrugia, 1999).
Dipotassium bismuth phosphate tungstate
top
Crystal data top
K2[Bi(PO4)(WO4)] | F(000) = 2192 |
Mr = 630 | Dx = 4.838 Mg m−3 |
Orthorhombic, Ibca | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -I 2b 2c | Cell parameters from 320 reflections |
a = 19.7253 (12) Å | θ = 15–23° |
b = 12.4764 (8) Å | µ = 34.77 mm−1 |
c = 7.0284 (2) Å | T = 293 K |
V = 1729.69 (16) Å3 | Prism, colorless |
Z = 8 | 0.08 × 0.07 × 0.03 mm |
Data collection top
Oxford XCalibur-3 CCD area-detector diffractometer | 1098 reflections with I > 2σ(I) |
φ and ω scans | Rint = 0.064 |
Absorption correction: multi-scan (Blessing, 1995) | θmax = 30°, θmin = 3.3° |
Tmin = 0.075, Tmax = 0.351 | h = −27→27 |
16151 measured reflections | k = −17→17 |
1265 independent reflections | l = −9→6 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0467P)2 + 34.3351P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.035 | (Δ/σ)max < 0.001 |
wR(F2) = 0.094 | Δρmax = 4.87 e Å−3 |
S = 1.18 | Δρmin = −2.37 e Å−3 |
1265 reflections | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
62 parameters | Extinction coefficient: 0.00034 (5) |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Bi | 0.25 | 0.58132 (3) | 0 | 0.01877 (16) | |
K | 0.09397 (11) | 0.82941 (18) | 0.2169 (3) | 0.0364 (5) | |
W | 0.08130 (2) | 0.5 | 0.25 | 0.02461 (17) | |
P | 0.25 | 0.8233 (2) | 0 | 0.0181 (5) | |
O1 | 0.2383 (3) | 0.9000 (4) | 0.1678 (9) | 0.0261 (12) | |
O2 | 0.3119 (3) | 0.7495 (5) | 0.0267 (8) | 0.0246 (11) | |
O3 | 0.1313 (3) | 0.5328 (5) | 0.0474 (10) | 0.0304 (13) | |
O4 | 0.0306 (4) | 0.3891 (6) | 0.1851 (13) | 0.0449 (17) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Bi | 0.0193 (2) | 0.0175 (2) | 0.0195 (2) | 0 | −0.00022 (13) | 0 |
K | 0.0239 (9) | 0.0481 (12) | 0.0373 (10) | 0.0068 (8) | 0.0007 (8) | −0.0019 (8) |
W | 0.0166 (2) | 0.0274 (2) | 0.0298 (3) | 0 | 0 | 0.00104 (17) |
P | 0.0222 (13) | 0.0138 (11) | 0.0181 (13) | 0 | 0.0006 (9) | 0 |
O1 | 0.043 (3) | 0.021 (2) | 0.014 (2) | −0.004 (2) | 0.004 (2) | −0.002 (2) |
O2 | 0.025 (3) | 0.020 (2) | 0.029 (3) | 0.001 (2) | −0.002 (2) | 0.004 (2) |
O3 | 0.023 (3) | 0.033 (3) | 0.035 (3) | −0.003 (2) | 0.003 (3) | 0.007 (3) |
O4 | 0.035 (4) | 0.050 (4) | 0.049 (4) | −0.020 (3) | −0.002 (3) | −0.001 (4) |
Geometric parameters (Å, º) top
Bi—O1i | 2.358 (6) | W—O4viii | 1.767 (7) |
Bi—O1ii | 2.358 (6) | W—O4 | 1.767 (7) |
Bi—O2 | 2.435 (6) | W—O3 | 1.780 (7) |
Bi—O2iii | 2.435 (6) | W—O3viii | 1.780 (7) |
Bi—O3 | 2.441 (6) | W—Kvii | 3.919 (2) |
Bi—O3iii | 2.441 (6) | W—Kiv | 3.919 (2) |
Bi—O1iv | 2.562 (6) | W—Kx | 4.067 (2) |
Bi—O1v | 2.562 (6) | W—Kxi | 4.067 (2) |
Bi—P | 3.019 (2) | W—Kviii | 4.124 (2) |
Bi—Ki | 3.830 (2) | P—O1 | 1.536 (6) |
Bi—Kii | 3.830 (2) | P—O1iii | 1.536 (6) |
K—O4vi | 2.658 (7) | P—O2iii | 1.541 (6) |
K—O2iii | 2.715 (6) | P—O2 | 1.541 (6) |
K—O2i | 2.768 (6) | P—Kiii | 3.435 (2) |
K—O3vii | 2.982 (7) | O1—Bii | 2.358 (6) |
K—O1 | 3.001 (7) | O1—Biix | 2.562 (6) |
K—O4viii | 3.078 (9) | O2—Kiii | 2.715 (6) |
K—O4ix | 3.179 (9) | O2—Ki | 2.768 (6) |
K—O3ix | 3.230 (7) | O3—Kii | 2.982 (7) |
K—P | 3.435 (2) | O3—Kiv | 3.230 (7) |
K—Bii | 3.830 (2) | O4—Kxi | 2.658 (7) |
K—Wix | 3.919 (2) | O4—Kviii | 3.078 (9) |
K—Kii | 4.034 (2) | O4—Kiv | 3.179 (9) |
| | | |
O1i—Bi—O1ii | 168.6 (3) | O3vii—K—O4ix | 130.9 (2) |
O1i—Bi—O2 | 77.85 (19) | O1—K—O4ix | 101.68 (19) |
O1ii—Bi—O2 | 92.30 (19) | O4viii—K—O4ix | 104.3 (2) |
O1i—Bi—O2iii | 92.30 (19) | O4vi—K—O3ix | 98.0 (2) |
O1ii—Bi—O2iii | 77.85 (19) | O2iii—K—O3ix | 76.70 (18) |
O2—Bi—O2iii | 61.0 (3) | O2i—K—O3ix | 120.06 (18) |
O1i—Bi—O3 | 89.0 (2) | O3vii—K—O3ix | 86.5 (2) |
O1ii—Bi—O3 | 93.8 (2) | O1—K—O3ix | 59.13 (17) |
O2—Bi—O3 | 133.2 (2) | O4viii—K—O3ix | 156.5 (2) |
O2iii—Bi—O3 | 75.1 (2) | O4ix—K—O3ix | 52.74 (17) |
O1i—Bi—O3iii | 93.8 (2) | O4viii—W—O4 | 111.0 (5) |
O1ii—Bi—O3iii | 89.0 (2) | O4viii—W—O3 | 109.9 (4) |
O2—Bi—O3iii | 75.1 (2) | O4—W—O3 | 106.7 (3) |
O2iii—Bi—O3iii | 133.2 (2) | O4viii—W—O3viii | 106.7 (3) |
O3—Bi—O3iii | 151.3 (3) | O4—W—O3viii | 109.9 (4) |
O1i—Bi—O1iv | 123.51 (16) | O3—W—O3viii | 112.7 (4) |
O1ii—Bi—O1iv | 67.8 (2) | O1—P—O1iii | 102.9 (5) |
O2—Bi—O1iv | 147.30 (19) | O1—P—O2iii | 110.3 (3) |
O2iii—Bi—O1iv | 132.88 (19) | O1iii—P—O2iii | 113.4 (3) |
O3—Bi—O1iv | 76.0 (2) | O1—P—O2 | 113.4 (3) |
O3iii—Bi—O1iv | 78.7 (2) | O1iii—P—O2 | 110.3 (3) |
O1i—Bi—O1v | 67.8 (2) | O2iii—P—O2 | 106.6 (4) |
O1ii—Bi—O1v | 123.51 (16) | P—O1—Bii | 143.8 (4) |
O2—Bi—O1v | 132.88 (19) | P—O1—Biix | 100.6 (3) |
O2iii—Bi—O1v | 147.30 (19) | Bii—O1—Biix | 111.1 (2) |
O3—Bi—O1v | 78.7 (2) | P—O1—K | 92.7 (3) |
O3iii—Bi—O1v | 76.0 (2) | Bii—O1—K | 90.44 (19) |
O1iv—Bi—O1v | 55.9 (3) | Biix—O1—K | 113.4 (2) |
O4vi—K—O2iii | 153.9 (2) | P—O2—Bi | 96.2 (3) |
O4vi—K—O2i | 123.4 (2) | P—O2—Kiii | 104.2 (3) |
O2iii—K—O2i | 79.72 (14) | Bi—O2—Kiii | 127.6 (2) |
O4vi—K—O3vii | 82.2 (2) | P—O2—Ki | 145.4 (3) |
O2iii—K—O3vii | 122.28 (18) | Bi—O2—Ki | 94.59 (19) |
O2i—K—O3vii | 62.11 (17) | Kiii—O2—Ki | 94.75 (19) |
O4vi—K—O1 | 145.6 (2) | W—O3—Bi | 134.3 (4) |
O2iii—K—O1 | 52.15 (17) | W—O3—Kii | 128.2 (3) |
O2i—K—O1 | 62.80 (17) | Bi—O3—Kii | 89.30 (19) |
O3vii—K—O1 | 71.70 (17) | W—O3—Kiv | 98.8 (2) |
O4vi—K—O4viii | 79.3 (2) | Bi—O3—Kiv | 109.6 (2) |
O2iii—K—O4viii | 95.38 (19) | Kii—O3—Kiv | 87.05 (19) |
O2i—K—O4viii | 79.2 (2) | W—O4—Kxi | 132.5 (4) |
O3vii—K—O4viii | 115.9 (2) | W—O4—Kviii | 113.9 (4) |
O1—K—O4viii | 132.18 (18) | Kxi—O4—Kviii | 94.0 (2) |
O4vi—K—O4ix | 78.52 (17) | W—O4—Kiv | 100.9 (3) |
O2iii—K—O4ix | 78.13 (19) | Kxi—O4—Kiv | 121.9 (3) |
O2i—K—O4ix | 157.8 (2) | Kviii—O4—Kiv | 80.3 (2) |
Symmetry codes: (i) −x+1/2, −y+3/2, −z+1/2; (ii) x, −y+3/2, z−1/2; (iii) −x+1/2, y, −z; (iv) x, y−1/2, −z; (v) −x+1/2, y−1/2, z; (vi) −x, y+1/2, −z+1/2; (vii) x, −y+3/2, z+1/2; (viii) x, −y+1, −z+1/2; (ix) x, y+1/2, −z; (x) −x, −y+3/2, z; (xi) −x, y−1/2, −z+1/2. |